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机构地区:[1]南京工业大学理学院,江苏南京210009 [2]南京中医药大学药学院,江苏南京210047 [3]西安交通大学医学院,陕西西安710061
出 处:《中国药业》2006年第16期14-16,共3页China Pharmaceuticals
摘 要:目的研究维拉帕米对映体在氨基甲酸酯类(ChiralcelOJ)手性柱上的拆分特性和规律。方法色谱柱为ChiralcelOJ手性柱(250mm×4.6mm,10μm),流动相为正己烷-无水乙醇-三乙胺,紫外检测波长为236nm。用溶质计量置换保留模型考察固定相和流动相中置换剂强度对拆分的影响,同时考察三乙胺及温度对保留与拆分的影响。结果维拉帕米对映体在选定色谱条件下均得到了基线分离,置换剂无水乙醇、三乙胺及温度对各对映体拆分有不同的影响,分离度在三乙胺浓度为0.6%、柱温为15℃时出现极大值。结论溶质计量置换保留模型的计量置换参数lgI和Z值,可以分别表征ChiralcelOJ柱的拆分能力和各对映体空间效应,适当增加三乙胺浓度和适当提高柱温可以改善和提高拆分效果。Objective To study the enantioselective characteristics and laws of Verapamil enantiomers on Chiralcel OJ column. Methods The experiments were performed under the HPLC conditions as following: the Chiralcel OJ column (250 mm ×4. 6 mm, 10 μm) as analytical column, mobile phase consisting of a mixture of n- hexane- ethanol- triethylamine, the detection wavelength at 236 nm and a flow rate of 0.5 mL/min. The effect of stationary phase and ethanol concentration in mobile phase on the enantiomer resolution were investigated by the stoichiometric displacement model for retention (SDM- R). So did as that of triethylamine concentration and the column temperature as well. Results Verapamil enantiomers were successfully separated on baseline under the selective condition. The ethanol in mobile phase, triethylamine and temperature would affect the resolution between Verapamil enantiomers. The resolution appeared a maximum value at 15℃ of column temperature and 0.6% of triethylamine concentration. Conclusion The lgl and Z values of SDM- R could be employed to characterize the resolution efficiency of Chiralcel OJ column and the specific effect of enantiomers interacted with the stationary phase. Adding tfiethylamine in mobile phase will increase the resolution efficacy and changing column temperature can promote enantiomer resolution.
关 键 词:维拉帕米 手性分离 溶质计量置换保留模型 纤维素氨基甲酸酯类手性柱
分 类 号:TQ460.72[医药卫生—药物分析学] R972.2[化学工程—制药化工]
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